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Hydrogen Bromide → p,p'-(Phenylphosphinylidene)bisphenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | Methyl Bromide | HCID 6323 | — |
| 反応物 | Sodium Sulfite | HCID 24437 | — |
| 反応物 | Potassium Bromide | HCID 253877 | — |
| 反応物 | Bis(4-methoxyphenyl)phenylphosphine oxide | HCID 4589182 | — |
| 生成物 | p,p'-(Phenylphosphinylidene)bisphenol | HCID 69930 | 74% |
反応手順
Bis(4-methoxyphenyl)phenylphosphine oxide mixture (2359 g, 6.97 mol), hydrobromic acid (48%, 8344 g, 49.5 mol), and potassium bromide (243 g, 2.04 mol) were stirred at 120° C. for 48 h. The flask was fitted with a sodium sulfite scrubber for containment of methyl bromide. The lower aqueous layer was removed and the product layer was worked up to afford bis(4-hydroxyphenyl)phenylphosphine oxide mixture (Composition VI) as a tan powder (1601 g, 74%). m.p. (DSC): 93° C. 31P NMR (d6-DMSO): δ 27.7 (s, 24.7%); 27.5 (s, 47.7%); 27.4 (s, 25.4%); 27.2 (s, 2.2%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07202311B2 |
| 出典データセット | uspto-grants-2007_04 |
| ORD ID | ord-d7bac0f34a684f858a5e1936117b0a03 |
| 出典メモ | uspto-grants-2007_04 |